CN109399722A - A kind of preparation method of porous rodlike molybdenum dioxide/carbon composite - Google Patents
A kind of preparation method of porous rodlike molybdenum dioxide/carbon composite Download PDFInfo
- Publication number
- CN109399722A CN109399722A CN201811609841.7A CN201811609841A CN109399722A CN 109399722 A CN109399722 A CN 109399722A CN 201811609841 A CN201811609841 A CN 201811609841A CN 109399722 A CN109399722 A CN 109399722A
- Authority
- CN
- China
- Prior art keywords
- molybdenum dioxide
- porous
- carbon composite
- preparation
- freeze
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation methods of porous rodlike molybdenum dioxide/carbon composite, first preparation Ammonium Molybdate Tetrahydrate aqueous solution；Then polyvinyl alcohol is added into Ammonium Molybdate Tetrahydrate aqueous solution, heating stirs to get mixed solution after stirring at normal temperature；After solution to be mixed is cooled to room temperature, freeze-drying obtains freeze-drying product；Finally the product of freeze-drying is calcined, arrives porous rodlike molybdenum dioxide/carbon composite after calcining.The method of the present invention preparation process is simple, reproducible, at low cost, and porous rodlike molybdenum dioxide/carbon composite of large specific surface area can be made.
Description
Technical field
The invention belongs to field of inorganic material preparing technology, and in particular to the porous rodlike molybdenum dioxide/carbon composite of one kind
Preparation method.
Background technique
Molybdenum dioxide is that a kind of resistivity is low, fusing point is high, thermal stability and the good transiting metal oxidation of chemical stability
Object.Because its unique structure and property molybdenum dioxide have extensively in fields such as photocatalysis, supercapacitor and lithium ion batteries
Application prospect.The disadvantages of few and easy to reunite there are active site for molybdenum dioxide, the composite material based on molybdenum dioxide
Preparation is known as research hotspot.Chinese invention patent CN106492820B discloses a kind of three-dimensional macroporous structure molybdenum dioxide load oxygen
Change the preparation method of cobalt granule；Chinese invention patent 102795667B discloses a kind of system of carbon-coated nano molybdenum dioxide material
Preparation Method；Chinese invention patent 106219616A disclose a kind of molybdenum dioxide/cobalt acid nickel classification hybrid nanostructure array and
Preparation method, the preparation method of foregoing invention have that technique is relative complex.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of porous rodlike molybdenum dioxide/carbon composite, to overcome
Defect of the existing technology, the method for the present invention preparation process is simple, reproducible, at low cost, and large specific surface area can be made
Porous rodlike molybdenum dioxide/carbon composite.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method of porous rodlike molybdenum dioxide/carbon composite, comprising the following steps:
Step 1: Ammonium Molybdate Tetrahydrate aqueous solution is prepared；
Step 2: polyvinyl alcohol being added into Ammonium Molybdate Tetrahydrate aqueous solution, and heating stirs to get mixing after stirring at normal temperature
Solution；
Step 3: after solution to be mixed is cooled to room temperature, freeze-drying obtains freeze-drying product；
Step 4: the product of freeze-drying is calcined, and arrives porous rodlike molybdenum dioxide/carbon after calcining
Composite material.
Further, the concentration of Ammonium Molybdate Tetrahydrate aqueous solution is 0.04mol/L in step 1.
Further, 5~25g polyvinyl alcohol is added in step 2 in every 200mL Ammonium Molybdate Tetrahydrate aqueous solution.
Further, the stirring at normal temperature time is 0.5h in step 2.
Further, heat up in step 2 stirring temperature be 85 DEG C, time 1h.
Further, the temperature being freeze-dried in step 3 is -40 DEG C, time 48h.
Further, it is calcined in step 4 specifically: the product of freeze-drying is put into tube furnace, under an inert atmosphere
700 DEG C of calcining 2h, and heating rate is 3 DEG C/min.
Compared with prior art, the invention has the following beneficial technical effects:
The preparation method of porous rodlike molybdenum dioxide/carbon composite of the invention, under the booster action of polyvinyl alcohol,
Molybdenum dioxide/carbon composite is obtained by calcining under freeze-drying and argon atmosphere.This method is easy to operate, at low cost, and two
The porous club shaped structure of molybdenum oxide/carbon composite effectively increases specific surface area, to can provide more active sites, makes
It obtains molybdenum dioxide/carbon composite and shows potential application value in catalysis and energy storage field.
Detailed description of the invention
Fig. 1 is 2 molybdenum dioxide of the embodiment of the present invention/carbon composite SEM figure, wherein (a) is amplification 1K, it (b) is to put
Big 10K；
Fig. 2 is 2 molybdenum dioxide of the embodiment of the present invention/carbon composite XRD diagram；
Fig. 3 is 2 molybdenum dioxide of the embodiment of the present invention/carbon composite Raman figure.
Specific embodiment
Embodiments of the present invention are described in further detail below:
A kind of preparation method of porous rodlike molybdenum dioxide/carbon composite, comprising the following steps:
1) the Ammonium Molybdate Tetrahydrate aqueous solution that 200mL concentration is 0.04mol/L is prepared.
2) 5~25g polyvinyl alcohol (1788 type) is added in the above solution, stirring at normal temperature 0.5h, then 85 DEG C of stirring 1h.
Etc. 3) after mixed solutions are cooling, 48h is freeze-dried at -40 DEG C.
4) product of freeze-drying being put into tube furnace, 700 DEG C of calcining 2h under atmosphere, heating rate is 3 DEG C/min,
After calcining, porous rodlike molybdenum dioxide/carbon composite is obtained.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
1) first step prepares the Ammonium Molybdate Tetrahydrate aqueous solution that 200mL concentration is 0.04mol/L.
2) 5g polyvinyl alcohol (1788 type) is added in the above solution in second step, stirring at normal temperature 0.5h, then 85 DEG C of stirrings
1h。
3) third step is freeze-dried 48h at -40 DEG C after waiting mixed solutions cooling.
4) product of freeze-drying is put into tube furnace by the 4th step, 700 DEG C of calcining 2h, heating rate 3 under atmosphere
DEG C/min, after calcining, obtain porous rodlike molybdenum dioxide/carbon composite.
Embodiment 2
1) first step prepares the Ammonium Molybdate Tetrahydrate aqueous solution that 200mL concentration is 0.04mol/L.
2) second step, is added 20g polyvinyl alcohol (1788 type) in the above solution, then stirring at normal temperature 0.5h is stirred for 85 DEG C
Mix 1h.
3) third step is freeze-dried 48h at -40 DEG C after waiting mixed solutions cooling.
4) product of freeze-drying is put into tube furnace by the 4th step, 700 DEG C of calcining 2h, heating rate 3 under atmosphere
DEG C/min, after calcining, obtain porous rodlike molybdenum dioxide/carbon composite.
Embodiment 3
1) first step prepares the Ammonium Molybdate Tetrahydrate aqueous solution that 200mL concentration is 0.04mol/L.
2) second step, is added 25g polyvinyl alcohol (1788 type) in the above solution, then stirring at normal temperature 0.5h is stirred for 85 DEG C
Mix 1h.
3) third step is freeze-dried 48h at -40 DEG C after waiting mixed solutions cooling.
4) product of freeze-drying is put into tube furnace by the 4th step, 700 DEG C of calcining 2h, heating rate 3 under atmosphere
DEG C/min, after calcining, obtain porous rodlike molybdenum dioxide/carbon composite.
Fig. 1 is that molybdenum dioxide/carbon composite SEM of embodiment 2 schemes.As can be seen from the figure obtained titanium dioxide
Molybdenum/carbon composite is micron-sized stub, and the inside and surface of stub have pore structure abundant, is conducive to improve material
Specific surface area and chemical property.
Fig. 2 is 2 molybdenum dioxide of embodiment/carbon composite XRD diagram.Main diffraction peak and molybdenum dioxide in figure
(PDF#32-0671) unanimously, and peak type is sharp, shows that molybdenum dioxide crystallinity and purity are all in molybdenum dioxide/carbon composite
It is high.
Fig. 3 is 2 molybdenum dioxide of embodiment/carbon composite Raman figure.As can be seen that in addition to the feature of molybdenum dioxide
Outside peak, there are also the characteristic peaks of apparent carbon, show that product is the composite material of molybdenum dioxide and carbon.
Claims (7)
1. a kind of preparation method of porous rodlike molybdenum dioxide/carbon composite, which comprises the following steps:
Step 1: Ammonium Molybdate Tetrahydrate aqueous solution is prepared；
Step 2: polyvinyl alcohol being added into Ammonium Molybdate Tetrahydrate aqueous solution, and heating stirs to get mixed solution after stirring at normal temperature；
Step 3: after solution to be mixed is cooled to room temperature, freeze-drying obtains freeze-drying product；
Step 4: the product of freeze-drying is calcined, to get compound to porous rodlike molybdenum dioxide/carbon after calcining
Material.
2. the preparation method of the porous rodlike molybdenum dioxide/carbon composite of one kind according to claim 1, feature exist
In the concentration of Ammonium Molybdate Tetrahydrate aqueous solution is 0.04mol/L in step 1.
3. the preparation method of the porous rodlike molybdenum dioxide/carbon composite of one kind according to claim 1, feature exist
In addition 5~25g polyvinyl alcohol in every 200mL Ammonium Molybdate Tetrahydrate aqueous solution in step 2.
4. the preparation method of the porous rodlike molybdenum dioxide/carbon composite of one kind according to claim 1, feature exist
In the stirring at normal temperature time is 0.5h in step 2.
5. the preparation method of the porous rodlike molybdenum dioxide/carbon composite of one kind according to claim 1, feature exist
In the temperature for the stirring that heats up in step 2 is 85 DEG C, time 1h.
6. the preparation method of the porous rodlike molybdenum dioxide/carbon composite of one kind according to claim 1, feature exist
In the temperature being freeze-dried in step 3 is -40 DEG C, time 48h.
7. the preparation method of the porous rodlike molybdenum dioxide/carbon composite of one kind according to claim 1, feature exist
In being calcined in step 4 specifically: the product of freeze-drying is put into tube furnace, under an inert atmosphere 700 DEG C of calcining 2h, and
Heating rate is 3 DEG C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811609841.7A CN109399722B (en) | 2018-12-27 | 2018-12-27 | Preparation method of porous rod-like molybdenum dioxide/carbon composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811609841.7A CN109399722B (en) | 2018-12-27 | 2018-12-27 | Preparation method of porous rod-like molybdenum dioxide/carbon composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109399722A true CN109399722A (en) | 2019-03-01 |
| CN109399722B CN109399722B (en) | 2020-10-30 |
Family
ID=65461525
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811609841.7A Active CN109399722B (en) | 2018-12-27 | 2018-12-27 | Preparation method of porous rod-like molybdenum dioxide/carbon composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109399722B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114232015A (en) * | 2022-01-10 | 2022-03-25 | 齐鲁工业大学 | Tubular MoO2Preparation and application of/C composite material |
| CN114743807A (en) * | 2022-05-19 | 2022-07-12 | 江苏大学 | Inside and outside raw MoO2Preparation method of/three-dimensional carbon composite material |
| CN115000370A (en) * | 2022-06-02 | 2022-09-02 | 烟台大学 | Molybdenum dioxide confinement growth and modification three-dimensional porous carbon composite electrode material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102623687A (en) * | 2012-04-09 | 2012-08-01 | 华中科技大学 | Preparation method for high-capacity molybdenum dioxide anode material and application of high-capacity molybdenum dioxide anode material |
| CN103288136A (en) * | 2012-02-27 | 2013-09-11 | 新疆教育学院 | Hydrothermal synthesis method of shape-controllable molybdenum dioxide submicrocrystals |
| CN106299259A (en) * | 2015-05-18 | 2017-01-04 | 韦升鸿 | The preparation method of a kind of molybdenum dioxide/carbon nano-particle and in the application of lithium ion battery |
| CN107394163A (en) * | 2017-07-25 | 2017-11-24 | 陕西科技大学 | A kind of copper molybdenum dioxide carbon composite of hollow core shell structure and its preparation method and application |
-
2018
- 2018-12-27 CN CN201811609841.7A patent/CN109399722B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288136A (en) * | 2012-02-27 | 2013-09-11 | 新疆教育学院 | Hydrothermal synthesis method of shape-controllable molybdenum dioxide submicrocrystals |
| CN102623687A (en) * | 2012-04-09 | 2012-08-01 | 华中科技大学 | Preparation method for high-capacity molybdenum dioxide anode material and application of high-capacity molybdenum dioxide anode material |
| CN106299259A (en) * | 2015-05-18 | 2017-01-04 | 韦升鸿 | The preparation method of a kind of molybdenum dioxide/carbon nano-particle and in the application of lithium ion battery |
| CN107394163A (en) * | 2017-07-25 | 2017-11-24 | 陕西科技大学 | A kind of copper molybdenum dioxide carbon composite of hollow core shell structure and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| LINZHOU ZHUANG等: "In-situ preparation of porous carbon-supported molybdenum dioxide and its performance in the oxidative desulfurization of thiophene", 《J MATER SCI》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114232015A (en) * | 2022-01-10 | 2022-03-25 | 齐鲁工业大学 | Tubular MoO2Preparation and application of/C composite material |
| CN114743807A (en) * | 2022-05-19 | 2022-07-12 | 江苏大学 | Inside and outside raw MoO2Preparation method of/three-dimensional carbon composite material |
| CN114743807B (en) * | 2022-05-19 | 2024-03-19 | 江苏大学 | Internally and externally generated MoO 2 Preparation method of three-dimensional carbon composite material |
| CN115000370A (en) * | 2022-06-02 | 2022-09-02 | 烟台大学 | Molybdenum dioxide confinement growth and modification three-dimensional porous carbon composite electrode material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109399722B (en) | 2020-10-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107195886B (en) | A kind of pyrophosphoric acid vanadium sodium@carbon composite anode material, preparation and application | |
| CN104475172B (en) | Preparation method and application of three-dimensional porous heteroatom-doped graphene | |
| CN109399722A (en) | A kind of preparation method of porous rodlike molybdenum dioxide/carbon composite | |
| CN104841469B (en) | A kind of preparation method of three-dimensional porous M N C catalysts | |
| CN104843708B (en) | A kind of preparation method of tungsten carbide hollow hemisphere | |
| CN110170331A (en) | A kind of hollow porous carbon ball nano material of iron nitrogen codope and preparation method thereof | |
| CN106711432B (en) | A kind of tridimensional network MoO2Nano material and its preparation and application | |
| CN106853375B (en) | The preparation method of the compound Electrocatalytic Activity for Hydrogen Evolution Reaction agent of the carbon-coated tungsten oxide/carbon of nitrogen phosphorus doping | |
| CN103700513B (en) | A kind of graphene paper and its preparation method and application | |
| CN109616671A (en) | A kind of method and application for preventing intermetallic compound from reuniting in high temperature and growing up | |
| CN108630947A (en) | A kind of preparation method of the cobalt sulfide of rechargeable type zinc-air battery/carbon nanocatalyst | |
| CN109665525B (en) | Preparation method of dumbbell-shaped iron-nitrogen double-doped porous carbon | |
| CN110433835A (en) | A kind of efficient liberation of hydrogen catalyst and preparation method thereof | |
| CN104843779B (en) | A kind of hollow ball-shape rutile titanium dioxide is mesomorphic and preparation method thereof | |
| CN102185147A (en) | Nano iron phosphate hollow sphere/graphene composite material and preparation method thereof | |
| CN109694051A (en) | It is graphitized the production method and its application of hollow carbon sphere and preparation method thereof and electrode material | |
| CN108807943B (en) | CeO with hollow structure2@ C core-shell nano composite material and preparation method and application thereof | |
| CN102500360A (en) | Method for preparing mesoporous tungsten oxide/carbon composite conductive materials | |
| CN105810960A (en) | Composite material taking foam nickel as matrix and preparation method of composite material | |
| CN104043453B (en) | A kind of support type cobaltosic oxide nano composite catalyst and application | |
| CN109473682B (en) | Supported binuclear perovskite type oxide carbon nano microsphere catalyst, and preparation method and application thereof | |
| CN107706397A (en) | Nickel-cobalt-manganese ternary combination electrode material of modified carbon nano-tube modification and preparation method thereof | |
| CN107935047B (en) | A kind of control synthetic method of different-shape and the nano-manganese dioxide of size | |
| CN113981489A (en) | Molybdenum carbide/carbon composite material, preparation method based on molten salt method and application | |
| CN106825553B (en) | A kind of preparation method of cobalt-nitrogen-carbon nucleocapsid hybrid hollow porous carbon ball |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220615 Address after: 710000 room 12001, floor 20, unit 1, building 1, Vanke Jinyu LANWAN, Chanba Third Road, Chanba Ecological District, Xi'an City, Shaanxi Province Patentee after: Xi'an tianniu Material Technology Co.,Ltd. Address before: No. 1, Weiyang District university garden, Xi'an, Shaanxi Province, Shaanxi Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY |
|
| TR01 | Transfer of patent right |